CN104161850A - Preparation method of Chinese herbal extract, prepared Chinese herbal extract and application - Google Patents
Preparation method of Chinese herbal extract, prepared Chinese herbal extract and application Download PDFInfo
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Abstract
The invention provides a preparation method of a Chinese herbal extract. Active pharmaceutical ingredients of the Chinese herbal extract comprise, by weight, 30-60 parts of Radix Astragali, 9-15 parts of ligustrum lucidum, 9-30 parts of motherwort, 3-10 parts of dark plum, 2-9 parts of coptis, 1-5 parts of cortex cinnamomi and 3-9 parts of Buddleja officinalis. The preparation method comprises the following steps: extracting volatile oil from cortex cinnamomi, and carrying out clathration on the volatile oil with beta-cyclodextrin; extracting Radix Astragali, ligustrum lucidum and Buddleja officinalis with 10%-100% (by volume) of an ethanol solution I; extracting dark plum, cortex cinnamomi herbal residue and herbal residues of Radix Astragali, ligustrum lucidum and Buddleja officinalis by the use of water; extracting motherwort and coptis with 10%-100% (by volume) of an ethanol solution II; and merging extracts and drying to obtain a dry extract powder, adding a volatile oil clathrate, and uniformly mixing. By the preparation method, active material content and pharmacological action of the Chinese herbal extract are boosted remarkably.
Description
Technical field
The invention belongs to the field of Chinese medicines, be specifically related to a kind of preparation method of the Chinese medicine extract for diabetic renal papillary necrosis and Chinese medicine extract and the purposes of preparation thereof.
Background technology
Diabetic renal papillary necrosis (Diabetic Retinopathy is called for short DR) is one of ocular complications that diabetes are serious and common.Along with the prolongation of diabetic duration, the incidence rate of DR also increases thereupon.In 8 years above persons of the course of disease, diabetic renal papillary necrosis incidence rate is about 50%.This disease early symptom is not obvious, easily out in the cold, and do not have again specific control method late period, and disease is touching, obstinate refractory.Primary disease loses to be controlled, and consequence is serious, is to cause the blind main cause of being grown up, and blind rate is up to 8-12%, and ill crowd's quality of life has been caused to serious harmful effect.Therefore, the control of DR has become current medical domain and has been badly in need of the great brainstorm subject solving, and is day by day subject to domestic and international medical circle and medical worker's great attention.But, still lack at present the active drug for the treatment of primary disease both at home and abroad.In order to meet the market demand of expanding day, prevent and delay the disease process of diabetic retinopathy, improve the quality of life of vast diabetics, the sick specialities of planting of advantage such as performance Chinese medicine difficult diseases, the new Chinese medicine of carrying out treatment DR has very important social meaning and economic worth.
(patent No. ZL200610087540.3 in applicant's " a kind of Chinese medicine preparation for the treatment of early diabetic retinopathy " patent by name in the early time, at 2009 Granted publication day JIUYUE 16 days), disclose a kind of Chinese medicine preparation for the treatment of early diabetic retinopathy, prescription consists of:
Radix Astragali 30-60g, Fructus Ligustri Lucidi 9-15g, Herba Leonuri 9-30g, Fructus Mume 3-10g, Rhizoma Coptidis 2-9g, Cortex Cinnamomi 2-5g, Flos Buddlejae 3-9g.
This patent document also discloses the preparation method of above-mentioned Chinese medicine preparation, that is: (1) gets seven doses of the various medicine components of corresponding proportioning; (2) with cleaning cold water soak 30 minutes; (3) put into boiling machine, add 2500 milliliters to soak water, decoct 40 minutes, mechanical presses goes out medicine juice; (4) in 14 sealed plastic bags of subpackage, 175 milliliters every bag.
Said method is only the simple preparation method of Chinese herbs decoction, does not consider how fully to extract the effective ingredient in medicine, brings dose large, and mouthfeel is poor, is inconvenient to carry the problem of unsuitable long term storage.
Therefore, on the basis of the difference of the active component that is necessary each herbal medicine in taking into full account prescription in kind, structure, physicochemical property, said extracted technique is optimized, to when reducing consumption, significantly improve drug effect, the medicine that provides better treatment of diabetic retinopathy to become for patient.
Summary of the invention
For the problems referred to above, one object of the present invention is to provide the preparation method of the Chinese medicine extract that a kind for the treatment of of diabetic retinopathy becomes.With the decocting cooking method comparison of prior art, the Chinese medicine extract that preparation method of the present invention prepares, the content of active substance is higher, drug effect is more remarkable.
In order to realize foregoing invention object, the present invention has adopted following technical scheme:
A preparation method for Chinese medicine extract, the crude drug of described Chinese medicine extract consists of:
Radix Astragali 30-60 weight portion, Fructus Ligustri Lucidi 9-15 weight portion, Herba Leonuri 9-30 weight portion, Fructus Mume 3-10 weight portion, Rhizoma Coptidis 2-9 weight portion, Cortex Cinnamomi 1-5 weight portion, Flos Buddlejae 3-9 weight portion;
Described preparation method comprises the steps:
(1) according to described weight portion, prepare each crude drug;
(2) Cortex Cinnamomi is extracted volatile oil, and Cortex Cinnamomi medicinal residues are standby, and volatile oil beta-cyclodextrin inclusion compound, obtains volatile oil clathrate compound;
(3) the alcoholic solution I that the Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae are 10%-100% with concentration of volume percent extracts, and ethanol extract reclaims ethanol, measures the extractum that relative density is 1.20-1.30 while being concentrated into 80 ℃, must extract extractum 1;
(4) the Cortex Cinnamomi medicinal residues that Fructus Mume and step (2) obtain, and step (2) Radix Astragali, Fructus Ligustri Lucidi and the Flos Buddlejae medicinal residues that obtain, with water extraction, aqueous extract adds the aqueous solution after the distillation that step (2) obtains, while being concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2;
(5) the alcoholic solution II that Herba Leonuri, Rhizoma Coptidis are 10%-100% with concentration of volume percent extracts, and ethanol extract reclaims ethanol, measures the extractum that relative density is 1.20-1.30 while being concentrated into 80 ℃, must extract extractum 3;
(6) will extract extractum 1,2,3 and merge, dry, spray dry or drying under reduced pressure, obtain dry extract, the described volatile oil clathrate compound that adds step (2) to obtain, and mix homogeneously, obtains.
Preferably, in described step (2), Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 6-16 times of medical material weight, extraction time is 3-7 hour.
Preferred, in described step (2), Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 8 times of medical material weight, 5 hours extraction times.
Also preferred, in described step (2), volatile oil is first used anhydrous alcohol solution, then carries out enclose with beta-schardinger dextrin-aqueous solution.
Preferred, in described step (2), the volume of described dehydrated alcohol is 1-3 times of volatile oil volume, more preferably 2 of volatile oil volume times.
Preferred, in described step (2), the weight of beta-schardinger dextrin-is 6-20 times of volatile oil volume, more preferably 10 of volatile oil volume times.
Preferred, in described step (2), described beta-schardinger dextrin-aqueous solution, water weight is 15-40 times of beta-schardinger dextrin-weight; Further preferred, the weight of water is 25 times of beta-schardinger dextrin-weight.
The preferred technical scheme of described step (2) is:
Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 6-16 times of Cortex Cinnamomi weight, extraction time is 3-7 hour; The another device of aqueous solution after distillation is collected, and Cortex Cinnamomi medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 1-3 times of volume, obtains volatile oil ethanol; Taking weight is volatile oil volume 6-20 beta-schardinger dextrin-doubly, adds beta-schardinger dextrin-weight 15-40 water doubly, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
The preferred technical scheme of described step (2) is:
Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 10 times of Cortex Cinnamomi weight, extraction time is 5 hours; The another device of aqueous solution after distillation is collected, and Cortex Cinnamomi medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 2 times of volumes, obtains volatile oil ethanol; Taking weight is the beta-schardinger dextrin-of 10 times of volatile oil volumes, adds the water of 25 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
Preferably, in described step (3), the concentration of volume percent of alcoholic solution I is 30%-80%, more preferably 70%.
Also preferred, in described step (3), the volume of alcoholic solution I is the described Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae medical material gross weight 6-14 times; Preferred, the volume of alcoholic solution I is the described Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae medical material gross weight 10 times.
Also preferred, in described step (3), extract 2-3 time each 0.5-2 hour; Preferred, extract each 1.5 hours 2 times.
Preferably, in described step (4), the weight of water is 6-16 times of medical material weight; Preferably, the weight of water is 8 times of medical material weight.
Also preferred, in described step (4), water extraction 1-3 time, each 1-3 hour; Preferred, water extraction 2 times, each 2 hours.
Preferably, in described step (5), the concentration of volume percent of alcoholic solution II is 30%-80%; Preferred, the concentration of volume percent of alcoholic solution II is 60%.
Also preferred, in described step (5), the volume of alcoholic solution II is 6-14 times of medical material weight; Preferred, the volume of alcoholic solution II is 10 times of medical material weight.
Also preferred, in described step (5), extract 2-3 time each 0.5-2 hour; Preferred, extract each 1.5 hours 3 times.
As a preferred embodiment of the present invention, the concrete operation step of described preparation method is as follows:
(1) according to described weight portion, prepare crude drug;
(2) Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 6-16 times of Cortex Cinnamomi weight, extraction time is 3-7 hour; The another device of aqueous solution after distillation is collected, and Cortex Cinnamomi medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 1-3 times of volume, obtains volatile oil ethanol; Taking weight is volatile oil volume 6-20 beta-schardinger dextrin-doubly, adds beta-schardinger dextrin-weight 15-40 water doubly, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose;
(3) the alcoholic solution I heating and refluxing extraction that the Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae are 30%-80% by the concentration expressed in percentage by volume that volume is medical material weight 6-14 times 2-3 time, each 0.5-2 hour, filter, merge ethanol extract each time, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1;
(4) the Cortex Cinnamomi medicinal residues that Fructus Mume and step (1) obtain, and step (2) Radix Astragali, Fructus Ligustri Lucidi and the Flos Buddlejae medicinal residues that obtain, with volume, be medical material weight 6-16 water heating and refluxing extraction doubly 1-3 time, each 1-3 hour, filters, merge filtrate each time, add the aqueous solution after the distillation that step (2) obtains, standing, filter, when filtrate is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2;
(5) Herba Leonuri, Rhizoma Coptidis are that the alcoholic solution II that medical material weight 6-14 concentration expressed in percentage by volume is doubly 30%-80% extracts 2-3 time with volume, each 0.5-2 hour, filter, merge ethanol extract each time, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 3;
(6) will extract extractum 1,2,3 and merge, spraying is dry, obtains dry extract, the described volatile oil clathrate compound that adds step (2) to obtain, and mix homogeneously, obtains.
As a preferred embodiment of the present invention, the concrete operation step of described preparation method is as follows:
(1) according to described weight portion, prepare crude drug;
(2) Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 10 times of Cortex Cinnamomi weight, extraction time is 5 hours; The another device of aqueous solution after distillation is collected, and Cortex Cinnamomi medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 2 times of volumes, obtains volatile oil ethanol; Taking weight is the beta-schardinger dextrin-of 10 times of volatile oil volumes, adds the water of 25 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose;
(3) the alcoholic solution I heating and refluxing extraction that the Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae are 70% by the concentration expressed in percentage by volume that volume is 10 times of medical material weight 2 times, each 1.5 hours, filter, merge ethanol extract twice, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1;
(4) the Cortex Cinnamomi medicinal residues that Fructus Mume and step (1) obtain, and step (2) Radix Astragali, Fructus Ligustri Lucidi and the Flos Buddlejae medicinal residues that obtain, with volume, be the water heating and refluxing extraction 2 times of 8 times of medical material weight, each 2 hours, filter, merge filtrate twice, add the aqueous solution after the distillation that step (2) obtains, standing, filter, when filtrate is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2;
(5) the alcoholic solution II that Herba Leonuri, Rhizoma Coptidis are 60% by the concentration expressed in percentage by volume that volume is 10 times of medical material weight extracts 3 times, each 1.5 hours, filter, merge three times ethanol extract, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 3;
(6) will extract extractum 1,2,3 and merge, spraying is dry, dry extract, and the described volatile oil clathrate compound that adds step (2) to obtain, mix homogeneously, obtains.
In above-mentioned preparation method, described crude drug composition is preferably:
Radix Astragali 30g, Fructus Ligustri Lucidi 15g, Herba Leonuri 15g, Fructus Mume 9g, Rhizoma Coptidis 6g, Cortex Cinnamomi 1g, Flos Buddlejae 6g.
The Chinese medicine extract that provides a kind of above-mentioned preparation method to prepare is provided another object of the present invention.
A further object of the invention is, the application of above-mentioned Chinese medicine extract in the medicine of preparation treatment of diabetic retinopathy change is provided.
In above-mentioned application, acceptable adjuvant pharmaceutically described in described Chinese medicine extract adds or do not add, is prepared into acceptable preparation clinically.
Pharmaceutically acceptable adjuvant of the present invention, can include but not limited to:
Diluent: be for example selected from one or more in starch, dextrin, pregelatinized Starch, lactose, microcrystalline Cellulose, calcium sulfate, calcium hydrogen phosphate, calcium carbonate, magnesium oxide, magnesium carbonate, gel aluminum hydroxide, beta-schardinger dextrin-, mannitol, sorbitol, methylcellulose, hydroxypropyl emthylcellulose, polyvinylpyrrolidone, Carboxymethyl cellulose sodium.
Binding agent: be for example selected from one or more in distilled water, ethanol, starch slurry, sodium carboxymethyl cellulose, hydroxypropyl cellulose, methylcellulose and ethyl cellulose, hypromellose.
Lubricant: be for example selected from one or more in Stepanol MG, Polyethylene Glycol, micropowder silica gel, magnesium stearate, Pulvis Talci.
Correctives: be for example selected from one or more of saccharin sodium, cyclamate, aspartame, stevioside and essence apoplexy due to endogenous wind.
Useful technique effect of the present invention is: (1) takes into full account the active component of each taste crude drug in prescription, adopts respectively Different Extraction Method and different solvents that crude drug is classified and extracted.Test example 1 shows, compares with traditional water decocting process, and preparation method of the present invention can make the extraction of each effective constituents of each medical material in prescription more complete, and the content that extracts effective ingredient in product is higher; Thereby for extract performance clinical therapeutic efficacy provides material base.(2) preparation method of the present invention, Cortex Cinnamomi is extracted separately volatile oil, and adopts beta-cyclodextrin inclusion compound volatile oil, not only in extract of the present invention, has retained volatile oil to greatest extent, and volatile oil stability improves.Have bibliographical information, Cortex Cinnamomi volatile oil has the effect of certain reduction blood glucose, and presents dose dependent.Therefore, the method for the invention, will be conducive to raising and the maintenance of described extract drug effect, and the water decoction of prior art, hardly containing volatile oil.
Pharmacodynamic experiment (test example 2) from improving diabetes rat hemorheology, retinal capillary morphology aspect proves, the extract that the method for the invention prepares under different technology conditions, the effect that improves diabetic retinal tissue in rat microangiopathies is all better than water decoction of the prior art, especially preferred embodiment 1, its effect more notable (P<0.01).Preparation method of the present invention is described, can significantly improves the therapeutic effect of extract.
Accompanying drawing explanation
Below, describe by reference to the accompanying drawings embodiment of the present invention in detail, wherein:
What the block diagram of Fig. 1 showed is in test example 1, the comparison of the Chinese herbs decoction of Chinese medicine extract of the present invention and prior art to main pharmacodynamics composition extraction ratio.
The specific embodiment
Referring to specific embodiment, the present invention is described.It will be appreciated by those skilled in the art that these embodiment are only for the present invention is described, the scope that it does not limit the present invention in any way.
Experimental technique in following embodiment, if no special instructions, is conventional method.In following embodiment, medicinal raw material used, reagent material etc., if no special instructions, be commercially available purchase product.
embodiment 1a kind of preparation method of Chinese medicine extract and the Chinese medicine extract of preparation thereof
Crude drug prescription:
Radix Astragali 6kg, Fructus Ligustri Lucidi 3kg, Herba Leonuri 3kg, Fructus Mume 1.8kg, Rhizoma Coptidis 1.2kg, Cortex Cinnamomi 0.2kg, Flos Buddlejae 1.2kg
The concrete steps of described preparation method are as follows:
(1) according to prescription, prepare ingredients.
(2) Cortex Cinnamomi adds the water of 10 times of medical material weight, uses extraction by steam distillation volatile oil, and the another device of aqueous solution after distillation is collected, and medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 2 times of volumes; Get 10 times of weight to the beta-schardinger dextrin-of volatile oil volume, add the beta-schardinger dextrin-aqueous solution that the water of 25 times of beta-schardinger dextrin-weight is made; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae add 70% alcohol reflux 2 times that volume is 10 times of medical material weight, each 1.5 hours, filter, merge ethanol extract twice, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1, medicinal residues are standby.
(4) Radix Astragali, Fructus Ligustri Lucidi and Flos Buddlejae medicinal residues and Fructus Mume that the Cortex Cinnamomi medicinal residues that step (2) obtains, step (3) obtain, the water reflux, extract, 2 times that adds 8 times of medical material gross weights, each 2 hours, filter, merge twice filtrate, add the aqueous solution after the distillation that step (2) obtains, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2.
(5) Herba Leonuri, Rhizoma Coptidis add 60% ethanol extraction 3 times that volume is 10 times of medical material gross weights, each 1.5 hours, filter, merge three times ethanol extract, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 3.
(6) will extract extractum 1,2,3 and merge, spraying is dry, and obtain and always extract extractum, the volatile oil clathrate compound that adds step 2 to obtain, mix homogeneously, obtains described Chinese medicine extract 4.42kg.
embodiment 2a kind of preparation method of Chinese medicine extract and the Chinese medicine extract of preparation thereof
Crude drug prescription:
Radix Astragali 6kg, Fructus Ligustri Lucidi 3kg, Herba Leonuri 3kg, Fructus Mume 1.8kg, Rhizoma Coptidis 1.2kg, Cortex Cinnamomi 0.2kg, Flos Buddlejae 1.2kg
The concrete steps of described preparation method are as follows:
(1) according to prescription, prepare ingredients.
(2) Cortex Cinnamomi adds the water of 8 times of medical material weight, uses extraction by steam distillation volatile oil, and the another device of aqueous solution after distillation is collected, and medicinal residues are standby; Volatile oil adds 1 times of volume anhydrous alcohol solution, gets 6 times of weight to the beta-schardinger dextrin-of volatile oil volume, adds the beta-schardinger dextrin-aqueous solution that the water of 15 times of beta-schardinger dextrin-weight is made; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae add 10% alcohol reflux 2 times that volume is 6 times of medical material gross weights, each 0.5 hour, filter, merge ethanol extract twice, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1, medicinal residues are standby.
(4) Radix Astragali, Fructus Ligustri Lucidi and Flos Buddlejae medicinal residues and Fructus Mume that the Cortex Cinnamomi medicinal residues that step (2) obtains, step (3) obtain, the water reflux, extract, 1 time that adds 6 times of medical material gross weights, extraction time is 1 hour, filter, filtrate adds the aqueous solution after the distillation that step (2) obtains, standing, filters, when filtrate decompression is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2.
(5) Herba Leonuri, Rhizoma Coptidis add 10% ethanol extraction 2 times that volume is 6 times of medical material gross weights, each 0.5 hour, filter, merge ethanol extract twice, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 3.
(6) will extract extractum 1,2,3 and merge, spraying is dry, and obtain and always extract extractum, the volatile oil clathrate compound that adds step 2 to obtain, mix homogeneously, obtains described Chinese medicine extract 4.28kg.
embodiment 3a kind of preparation method of Chinese medicine extract and the Chinese medicine extract of preparation thereof
Crude drug prescription:
Radix Astragali 6kg, Fructus Ligustri Lucidi 3kg, Herba Leonuri 3kg, Fructus Mume 1.8kg, Rhizoma Coptidis 1.2kg, Cortex Cinnamomi 0.2kg, Flos Buddlejae 1.2kg
The concrete steps of described preparation method are as follows:
(1) according to prescription, prepare ingredients.
(2) Cortex Cinnamomi adds the water of 12 times of medical material weight, uses extraction by steam distillation volatile oil, and the another device of aqueous solution after distillation is collected, and medicinal residues are standby; Volatile oil adds 3 times of volume anhydrous alcohol solutions, gets 20 times of weight to the beta-schardinger dextrin-of volatile oil volume, adds the beta-schardinger dextrin-aqueous solution that the water of 40 times of beta-schardinger dextrin-weight is made; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae add 100% alcohol reflux 3 times that volume is 14 times of medical material gross weights, each 2 hours, filter, merge three times ethanol extract, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1, medicinal residues are standby.
(4) Radix Astragali, Fructus Ligustri Lucidi and Flos Buddlejae medicinal residues and Fructus Mume that the Cortex Cinnamomi medicinal residues that step (2) obtains, step (3) obtain, the water reflux, extract, 3 times that adds 16 times of medical material gross weights, each 3 hours, filter, merge three times filtrate, add the aqueous solution after the distillation that step (2) obtains, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2.
(5) Herba Leonuri, Rhizoma Coptidis add 100% ethanol extraction 3 times that volume is 14 times of medical material gross weights, each 2 hours, filter, merge three times ethanol extract, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 3.
(6) will extract extractum 1,2,3 and merge, spraying is dry, and obtain and always extract extractum, the volatile oil clathrate compound that adds step 2 to obtain, mix homogeneously, obtains described Chinese medicine extract 4.02kg.
embodiment 4a kind of preparation method of Chinese medicine extract and the Chinese medicine extract of preparation thereof
Crude drug prescription "
Radix Astragali 6kg, Fructus Ligustri Lucidi 3kg, Herba Leonuri 3kg, Fructus Mume 1.8kg, Rhizoma Coptidis 1.2kg, Cortex Cinnamomi 0.2kg, Flos Buddlejae 1.2kg
The concrete steps of described preparation method are:
(1) according to prescription, prepare ingredients.
(2) Cortex Cinnamomi, adds the water of 8 times of medical material weight, uses extraction by steam distillation volatile oil, and the another device of aqueous solution after distillation is collected, and medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 2 times of volumes; Get 20 times of weight to the beta-schardinger dextrin-of volatile oil volume, add the beta-schardinger dextrin-aqueous solution that the water of 30 times of beta-schardinger dextrin-weight is made; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae add 30% alcohol reflux 2 times of 12 times of medical material gross weights, each 2 hours, filter, merge ethanol extract twice, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1, medicinal residues are standby;
(4) Radix Astragali, Fructus Ligustri Lucidi and Flos Buddlejae medicinal residues and Fructus Mume that the Cortex Cinnamomi medicinal residues that step (2) obtains, step (3) obtain, the water reflux, extract, 3 times that adds 10 times of medical material gross weights, each 1 hour, filter, merge three times filtrate, add the aqueous solution after the distillation that step (2) obtains, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2;
(5) Herba Leonuri, Rhizoma Coptidis add 30% ethanol extraction 3 times of 8 times of medical material gross weights, and each 1 hour, filter, merges three times ethanol extract, recovery ethanol, measures the extractum that relative density is 1.20-1.30 while being evaporated to 80 ℃, must extract extractum 3;
(6) will extract extractum 1,2,3 and merge, spraying is dry, and obtain and always extract extractum, the volatile oil clathrate compound that adds step 2 to obtain, mix homogeneously, obtains described Chinese medicine extract 4.45kg.
embodiment 5a kind of preparation method of Chinese medicine extract and the Chinese medicine extract of preparation thereof
Crude drug prescription:
Radix Astragali 6kg, Fructus Ligustri Lucidi 3kg, Herba Leonuri 3kg, Fructus Mume 1.8kg, Rhizoma Coptidis 1.2kg, Cortex Cinnamomi 0.2kg, Flos Buddlejae 1.2kg
The concrete steps of described preparation method are:
(1) according to prescription, prepare ingredients.
(2) Cortex Cinnamomi adds the water of 12 times of medical material volumes, uses extraction by steam distillation volatile oil, and the another device of aqueous solution after distillation is collected, and medicinal residues are standby; Volatile oil adds 2 times of amount anhydrous alcohol solutions, gets 9 times of weight to the beta-schardinger dextrin-of volatile oil volume, adds the beta-schardinger dextrin-aqueous solution that the water of 35 times of beta-schardinger dextrin-weight is made; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae add 80% alcohol reflux 3 times of 8 times of medical material gross weights, each 0.5 hour, filter, merge three times ethanol extract, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1, medicinal residues are standby;
(4) Radix Astragali, Fructus Ligustri Lucidi and Flos Buddlejae medicinal residues and Fructus Mume that the Cortex Cinnamomi medicinal residues that step (2) obtains, step (3) obtain, the water reflux, extract, 1 time that adds 12 times of medical material gross weights, extraction time is 3 hours, filter, add the aqueous solution after the distillation that step (2) obtains, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2;
(5) Herba Leonuri, Rhizoma Coptidis add 80% ethanol extraction 3 times of 10 times of medical material gross weights, and each 1 hour, filter, merges three times ethanol extract, recovery ethanol, measures the extractum that relative density is 1.20-1.30 while being evaporated to 80 ℃, must extract extractum 3;
(6) will extract extractum 1,2,3 and merge, spraying is dry, and obtain and always extract extractum, the volatile oil clathrate compound that adds step 2 to obtain, mix homogeneously, obtains described Chinese medicine extract 4.36kg.
comparative example 1a kind of preparation method of Chinese medicine composition and the Chinese herbs decoction of preparation thereof
Crude drug prescription:
Radix Astragali 6kg, Fructus Ligustri Lucidi 3kg, Herba Leonuri 3kg, Fructus Mume 1.8kg, Rhizoma Coptidis 1.2kg, Cortex Cinnamomi 0.2kg, Flos Buddlejae 1.2kg
The preparation method of described Chinese medicine composition, concrete steps are:
(1) according to prescription, prepare ingredients.
(2) get ingredients, with cleaning cold water soak 30 minutes, put into boiling machine, add 71.43 liters to soak water, decoct 40 minutes, mechanical presses goes out medicine juice, is evaporated to 18.74 liters, obtains described Chinese herbs decoction; Then spraying is dry, obtains dry extract 4.16kg.
test example 1the comparison of the Chinese herbs decoction of Chinese medicine extract of the present invention and prior art
Test sample:
1) Chinese medicine extract that prepared by embodiment of the present invention 1-5
2) dry extract of the Chinese herbs decoction that prepared by comparative example
Test method:
1) assay of astragaloside
Chromatographic condition: take octadecylsilane chemically bonded silica as filler; The acetonitrile-water (35:65) of take is mobile phase; Evaporative light scattering detector detects.
The preparation of reference substance solution: get astragaloside reference substance appropriate, accurately weighed, add methanol and make every 1ml containing the solution of 0.3mg, obtain.
The preparation of need testing solution: get test sample 3g, accurately weighed, precision adds methanol 100ml, weighed weight, reflux 1 hour, lets cool, weighed weight, supplies weight with methanol again, shakes up, filter, discard just filtrate, the accurate subsequent filtrate 50ml that draws, evaporate to dryness, adds water 25ml and makes to dissolve, and with water-saturated n-butanol jolting, extracts 4 times, each 25ml, merges n-butyl alcohol, with ammonia solution, fully washs 3 times, each 40ml, discard ammoniacal liquor, n-butyl alcohol liquid evaporate to dryness, residue adds dissolve with methanol, be transferred in 5ml measuring bottle, add methanol to scale, shake up, obtain.
The preparation of medical material need testing solution: by " preparation of need testing solution " method preparation under version < < Chinese Pharmacopoeia > 283 pages of Milkvetch Roots of > [assay] item in 2010.
Algoscopy: precision is drawn reference substance solution 10 μ l, 30 μ l respectively, need testing solution 20 μ l, injection liquid chromatography, measures, and with external standard two-point method logarithmic equation, calculates, and obtains.
In extraction ratio=astragaloside total amount/input medical material, contain astragaloside total amount * 100%
2) assay of linarin
Chromatographic condition: take octadecylsilane chemically bonded silica as filler, the methanol-water-acetic acid (45:54.5:0.5) of take is mobile phase, and detection wavelength is 326nm.
The preparation of reference substance solution: get linarin reference substance appropriate, accurately weighed, add methanol and make every 1ml containing the solution of 0.3mg, obtain.
The preparation of need testing solution: get test sample 1g, accurately weighed, precision adds 50% ethanol 50ml, weighed weight, supersound process 30 minutes, lets cool, more weighed weight, with 50% methanol, supplies weight, shakes up, and filters, and gets subsequent filtrate, obtains.
The preparation of medical material need testing solution: by " preparation of need testing solution " method preparation under version < < Chinese Pharmacopoeia > 308 pages of Flos Buddlejae medical materials of > [assay] item in 2010.Algoscopy: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and injection liquid chromatography, measures, and obtains.
In extraction ratio=linarin total amount/input medical material, contain linarin total amount * 100%
3) assay of berberine
Chromatographic condition: take octadecylsilane chemically bonded silica as filler, with acetonitrile-0.05mol/L potassium dihydrogen phosphate (50:50), (every 100ml adds sodium lauryl sulphate 0.4g, take phosphorus acid for adjusting pH value as 4.0 again) be mobile phase, detection wavelength is 345nm
The preparation of reference substance solution: get berberine hydrochloride reference substance appropriate, accurately weighed, add methanol and make every 1ml containing the solution of 0.1mg, obtain.
The preparation of need testing solution: get test sample 0.3g, accurately weighed, precision adds methanol 50ml, weighed weight, supersound process 30 minutes, lets cool, more weighed weight, supplies the weight of less loss with methanol, shakes up, and filters, and gets subsequent filtrate, obtains.
The preparation of medical material need testing solution: by " preparation of need testing solution " method preparation under version < < Chinese Pharmacopoeia > 285 pages of Rhizoma Coptidis of > [assay] item in 2010.
Algoscopy: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and injection liquid chromatography, measures, and obtains.
In extraction ratio=berberine total amount/input medical material, contain berberine total amount * 100%
4) assay of leonurine
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filler, and 0.1% phosphoric acid solution (24:76) of acetonitrile-0.4% perfluorooctane sulfonate of take is mobile phase, and detection wavelength is 277nm.
The preparation of reference substance solution: get leonurine reference substance appropriate, accurately weighed, add methanol and make every 1ml containing the solution of 0.03mg, in contrast product solution.
The preparation of need testing solution: get test sample 2g, accurately weighed, precision adds 75% methanol 25ml, weighed weight, supersound process 30 minutes, lets cool, more weighed weight, supplies the weight of less loss with 75% methanol, shakes up, and filters, and gets subsequent filtrate, obtains.
The preparation of medical material need testing solution: by " preparation of need testing solution " method preparation under version < < Chinese Pharmacopoeia > 272 pages of Herba Leonuri medical materials of > [assay] item in 2010.
Algoscopy: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and injection liquid chromatography, measures, and obtains.
In extraction ratio=leonurine total amount/input medical material, contain leonurine total amount * 100%
5) assay of cinnamic aldehyde
Chromatographic condition: take octadecylsilane chemically bonded silica as filler; The acetonitrile-water (35:75) of take is mobile phase; Detection wavelength is 290nm.
The preparation of reference substance solution: get cinnamic aldehyde reference substance appropriate, accurately weighed, add methanol and make every 1ml containing the solution of l0 μ g, obtain.
The preparation of need testing solution: get test sample 0.5g, accurately weighed, put in tool plug conical flask, precision adds methanol 25ml, weighed weight, supersound process (power 350W, frequency 35kHz) 10 minutes, placement is spent the night, with method supersound process once, more weighed weight, with methanol, supply the weight of less loss, shake up, filter, obtain.
The preparation of medical material need testing solution: by " preparation of need testing solution " method preparation under version < < Chinese Pharmacopoeia > 127 pages of Cortex Cinnamomi medical materials of > [assay] item in 2010.
Algoscopy: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and injection liquid chromatography, measures, and obtains.
In extraction ratio=cinnamic aldehyde total amount/input medical material, contain cinnamic aldehyde total amount * 100%
Result of the test: in Table 1 and Fig. 1.
1) table 1 shows, preparation method of the present invention, the extract of preparing under different technical parameters, the compositions of the comparative example that the extraction ratio of each composition of detection is all write out a prescription higher than same materials medicine; Especially cinnamic aldehyde is not measured in the water decoction dry extract of comparative example.
2) extraction ratio of embodiment 1 pair of astragaloside, linarin and berberine is higher than other embodiment.
Conclusion (of pressure testing):
1) preparation method of the present invention can significantly be improved the extraction efficiency of prior art, makes Chinese medicine extract prepared by the present invention when clinical practice, have pharmacodynamic substances basis more reliably.
2) astragaloside, linarin and berberine are the effective ingredient for the treatment of diabetes and diabetic renal papillary necrosis.Described in embodiment 1 preparation method to the extraction ratio of above-mentioned three kinds of compositions the preparation method apparently higher than other embodiment, illustrate that the preparation method described in embodiment 1 is the preferred method of the present invention.
Table 1 comparative example and embodiment active ingredient contrast table
test example 2the impact of Chinese medicine extract of the present invention on the diabetic retinal tissue in rat pathological changes of STZ induction
Diabetic renal papillary necrosis is the optical fundus microangiopathies that diabetes long-run development causes, and its main pathological change is because long-term hyperglycemia directly or indirectly affects its hemorheological property, finally causes damage and the changing function of retinal blood tubular construction.The diabetes rat model of STZ induction is more generally acknowledged diabetes model in the world at present, after modeling for a long time, progressively forms diabetic renal papillary necrosis.This test adopts the method for an abdominal cavity note STZ to prepare diabetes rat model, the impact on diabetic retinal tissue in rat microangiopathies by pharmaceutical intervention preparation method more of the present invention and the prepared extract of prior art.
1, experimental technique
1.1 animal groupings
Get SPF level SD rat, adaptability was raised after 1 week, was divided at random 2 groups: blank group (15), diabetic groups (120).After all animal fasting 16h, the 0.01mol/L of blank group rats by intraperitoneal injection (i.p.) 55mg/kg, pH4.4 citrate buffer solution; Diabetes rats lumbar injection 1%STZ55mg/kg (being temporarily dissolved in 0.01mol/L, in the citrate buffer solution of pH4.4).Modeling is tail venous blood sampling survey fasting glucose after 1 week, take blood glucose >=16.7mmol/L as model success standard.The below standard rat of blood glucose is added STZ40mg/kg again, again detects its fasting glucose after 7 days, screens the successful rat of twice modeling (twice success rate is 88%).The rat that meets diabetes standard is divided into 7 groups more at random by blood glucose, body weight level, model group, 1 group of embodiment, 2 groups of embodiment, 3 groups of embodiment, 4 groups of embodiment, 5 groups of embodiment, comparative example group, 15 every group.
This prescription people with dosage is: people every day is with crude drug amount 82g/60kg, i.e. 1.4g/kg.According to conversion factor table, finding rat body weight conversion factor is 6.25, and the dose,equivalent of conversion rat is 6.25 * 1.4g/kg=8.75g/kg, i.e. 8.75g crude drug amount/kg.Except model group, it is all 8.75g crude drug amount/kg that the dosage of each group is converted to crude drug.
1.2 pharmaceutical intervention
1 group of (extract that embodiment 1 prepares of embodiment, add deionized water and make the solution of 0.236g/ml, dosage: 10ml/kg), 2 groups of (extracts that embodiment 2 prepares of embodiment, add deionized water and make the solution of 0.228g/ml, dosage: 10ml/kg), 3 groups of (extracts that embodiment 3 prepares of embodiment, add deionized water and make the solution of 0.214g/ml, dosage: 10ml/kg), 4 groups of (extracts that embodiment 4 prepares of embodiment, add deionized water and make the solution of 0.237g/ml, dosage: 10ml/kg), 5 groups of (extracts that embodiment 5 prepares of embodiment, add deionized water and make the solution of 0.233g/ml, dosage: 10ml/kg), comparative example group (the pharmaceutical composition that comparative example prepares, add deionized water and make the solution of 0.222g/ml, dosage: 10ml/kg), model group and blank group give the deionized water of respective volume, gastric infusion, administration every day 1 time, administration is 3 months altogether.During administration, give sufficient drinking-water, food, change bedding and padding every day.
1.3 indexs detect
1.3.1 hemorheology detects
When experiment finishes, rat aorta is got blood, anticoagulant heparin, and 3000r/min, centrifugal 15min, leaves and takes blood plasma.With blood viscosity instrument, measure whole blood viscosity and the plasma viscosity under different shear rates; By red blood cell deformation, assemble instrument and measure erythrocyte aggregation index, experimental result is in Table 2.
1.3.2 retinal capillary morphological change
Adopt rat retina surface preparation technic to observe its retinal capillary morphological change.After rat anesthesia, with normal saline, through heart perfusion, rinse blood, when eyeball from ruddy become pale after, win the eyeball with optic nerve, be fixed on 4 ℃ of 4%PFA48-72h.From 4%PFA, take out eyeball, flowing water rinses 10min gently, puts into the culture dish that fills PBS; From corpus ciliare rear portion along pot tip edge annular, cut off sclera, remove cornea and crystalline lens, rear eyecup Fructus Citri tangerinae lobe sample centered by depending on nipple is cut into 3, careful separation goes out retina; PBS (0.01mol/L pH7.4) rinsing l0min, is placed in 0.15mol/L pH7.4 glycine buffer soaked overnight; 3% trypsin matching while using) 37 ℃ of air bath agitators digestion retina 2-4h, observe at any time, treat that internal limiting membrane edge floats, and are about to when separated, stop digestion with retina remainder; Shift retina in 0.1MPBS, inhale gently to blow down and remove internal limiting membrane, then featheriness repeatedly, inhale and beat, the vasoganglion of remaining layer of transparent only, floats and gets and be laid in anticreep and carry on the sheet of slope, puts after natural drying at room temperature, deposit in 4 ℃ of section boxes and dye in order to PAS, neutral gum sealing, standby.
2, experimental result
2.1 each processed group are on the hemorheological impact of diabetes rat
2.1.1 with the comparison of blank group, the erythrocyte aggregation index of model group rat, whole blood viscosity (height cuts, in cut, low cutting), plasma viscosity level all significantly increases (P<0.01), illustrate that modeling successfully.
2.1.2 with model group comparison, the erythrocyte aggregation index of 1,2,3,4,5 groups of embodiment and comparative example group, whole blood viscosity (in cut, low cutting), plasma viscosity level all significantly or extremely significantly reduce (P<0.05 or P<0.01), wherein the decline of every detection index of 1,4,5 groups of embodiment is more remarkable, and decline degree is all greater than comparative example group.1 group of embodiment and the comparison of comparative example group, have utmost point significant difference (P<0.01); 4,5 groups of embodiment and the comparison of comparative example group, have significant difference (P<0.05).The big or small sequence of each group effect is: 2 groups of > comparative example groups of 3 groups of > embodiment of 4 groups of > embodiment of 5 groups of > embodiment of 1 group of > embodiment of embodiment.
Embodiment 1-5 is identical with the crude drug prescription of comparative example, and difference is preparation method, and the difference of the extract being caused by different preparation methoies.The extract that preparation method of the present invention prepares is better than water decoction prepared by prior art in the effect improving aspect diabetes rat hemorheology.Therefore, preparation method of the present invention is the reason place of improving curative effect of medication.The improvement of preparation method just, just drug action is significantly improved.Especially, the therapeutic effect of the extract of embodiment 1 preparation is obviously better than other each embodiment group.Therefore, the preparation method of embodiment 1 is that the present invention is most preferred, is secondly the preparation method of embodiment 5 and embodiment 4.
Table 2 is on the hemorheological impact of diabetes rat
Note: "
*" represent to compare with blank group p<0.01; "
#" represent to compare with model group, p<0.05, "
##" represent to compare with model group p<0.01; "
▲" represent to compare with comparative example group, p<0.05, "
▲ ▲" represent to compare with comparative example group p<0.01.
2.2 each processed group are on the morphologic impact of rat retina blood capillary
Through retina paving sheet, read sheet analysis, each processed group rat retina blood capillary morphological observation result is as follows:
Blank group: the retinal capillary of rat is distributed with rule, moves towards soft, caliber even thickness; Retina arteriovenous is through wherein, and tremulous pulse dyeing is darker, and vein dyeing is more shallow; Endotheliocyte is positioned at the central authorities of blood capillary, and core is larger, dyes more shallow; Pericyte is positioned at the tube chamber outside of blood capillary, and core is less, dyes darker.
Model group: rat retina blood capillary is arranged extremely disorderly, moves towards very irregular; Not etc., or sections do not expand or degenerates part blood capillary tube chamber thickness, is the expansion of capsule sample, or blood vessel degenerates, and tube chamber locking, forms acellular capillary, occurs without perfusion area; The dry sclerosis situation of blood vessel is obvious; Retinal vein expansion phenomenon is obvious; While pericyte's decreased number.But have no capillary hemangioma.
With model group comparison, the retinal capillary of the rat of comparative example group is moved towards irregular phenomenon and is obviously reduced, and pericyte's number increases, acellular capillary decreased number.
With model group comparison, the retinal capillary of the rat of 2,3 groups of comparative example groups of embodiment is moved towards irregular phenomenon and is obviously reduced, and pericyte's number increases, acellular capillary decreased number.The retinal capillary of 1,4,5 groups of rats of embodiment is moved towards normal, and pericyte's number increases, acellular capillary decreased number, and the quantity of minimizing is all better than comparative example group.
Therefore, the Chinese medicine extract that preparation method of the present invention prepares is improved effect to diabetic retinal tissue in rat microangiopathies, and is better than decoct prepared by prior art.Illustrate that the improvement of preparation method has significantly improved the pharmacological action of compound.
In a word, the pharmacy digital proof of test example 1, in the Chinese medicine extract of embodiment 1,2,3,4,5 prepared by the method for the invention, the content of effective substance is higher than existing preparation technology's the corresponding composition of water decoction.From determining the angle on the pharmacodynamic substances basis of drug effect power, the present invention designs and passes through according to the feature of each medical material the preparation technology that the extraction process of optimizing is better than water decoction.
In addition, the effect experiment result of test example 2 also proves, the Chinese medicine extract of embodiment 1,2,3,4,5 prepared by the method for the invention is all better than water decoction group prepared by prior art to diabetes rat hemorheology and the morphologic improvement effect of retinal capillary, illustrate that extract that preparation method of the present invention prepares is improved the effect of diabetic retinal tissue in rat microangiopathies, and be better than water decoction prepared by prior art, technology of preparing of the present invention has significantly improved the pharmacological action of compound.
embodiment 6a kind of Chinese medicine granules
Crude drug prescription:
Radix Astragali 6kg, Fructus Ligustri Lucidi 3kg, Herba Leonuri 3kg, Fructus Mume 1.8kg, Rhizoma Coptidis 1.2kg, Cortex Cinnamomi 0.2kg, Flos Buddlejae 1.2kg
According to preparation method step (1)-(5) described in embodiment 1, prepare volatile oil clathrate compound, extract extractum 1,2,3; United extraction extractum 1,2,3, obtains always extracting extractum, with dextrin 1.58kg, aspartame 30g, adopts the method for spray granulation, granulation, the volatile oil clathrate compound that adds step (2) to obtain, obtains granule 6kg, pack, every bag of 5g, makes 1200 bags altogether.
Specific description of embodiments of the present invention above does not limit the present invention, and those skilled in the art can make according to the present invention various changes or distortion, only otherwise depart from spirit of the present invention, all should belong to the scope of claims of the present invention.
Claims (10)
1. a preparation method for Chinese medicine extract, the crude drug of described Chinese medicine extract consists of:
Radix Astragali 30-60 weight portion, Fructus Ligustri Lucidi 9-15 weight portion, Herba Leonuri 9-30 weight portion, Fructus Mume 3-10 weight portion, Rhizoma Coptidis 2-9 weight portion, Cortex Cinnamomi 1-5 weight portion, Flos Buddlejae 3-9 weight portion;
It is characterized in that, described preparation method comprises the steps:
(1) according to described weight portion, prepare each crude drug;
(2) Cortex Cinnamomi is extracted volatile oil, and Cortex Cinnamomi medicinal residues are standby, and volatile oil beta-cyclodextrin inclusion compound, obtains volatile oil clathrate compound;
(3) the alcoholic solution I that the Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae are 10%-100% with concentration of volume percent extracts, and ethanol extract reclaims ethanol, measures the extractum that relative density is 1.20-1.30 while being concentrated into 80 ℃, must extract extractum 1;
(4) the Cortex Cinnamomi medicinal residues that Fructus Mume and step (1) obtain, and step (2) Radix Astragali, Fructus Ligustri Lucidi and the Flos Buddlejae medicinal residues that obtain, with water extraction, aqueous extract adds the aqueous solution after the distillation that step (2) obtains, while being concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2;
(5) the alcoholic solution II that Herba Leonuri, Rhizoma Coptidis are 10%-100% with concentration of volume percent extracts, and ethanol extract reclaims ethanol, measures the extractum that relative density is 1.20-1.30 while being concentrated into 80 ℃, must extract extractum 3;
(6) will extract extractum 1,2,3 and merge, oven dry, drying under reduced pressure or spraying are dry, and obtain and always extract extract powder, the described volatile oil clathrate compound that adds step (2) to obtain, mix homogeneously, obtains.
2. preparation method according to claim 1, is characterized in that, in described step (2), and Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 6-16 times of medical material weight, extraction time is 3-7 hour; Preferably, the weight of water is 8 times of medical material weight, 5 hours extraction times;
Preferably, in described step (2), volatile oil is first used anhydrous alcohol solution, then carries out enclose with beta-schardinger dextrin-aqueous solution;
Preferred, in described step (2), the volume of described dehydrated alcohol is 1-3 times of volatile oil volume, more preferably 2 of volatile oil volume times;
Preferred, in described step (2), the weight of beta-schardinger dextrin-is 6-20 times of volatile oil volume, more preferably 10 of volatile oil volume times;
Preferred, in described step (2), described beta-schardinger dextrin-aqueous solution, water weight is 15-40 times of beta-schardinger dextrin-weight; Further preferred, the weight of water is 25 times of beta-schardinger dextrin-weight.
3. preparation method according to claim 2, is characterized in that, the technical scheme of described step (2) is:
Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 6-16 times of Cortex Cinnamomi weight, extraction time is 3-7 hour; The another device of aqueous solution after distillation is collected, and Cortex Cinnamomi medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 1-3 times of volume, obtains volatile oil ethanol; Taking weight is volatile oil volume 6-20 beta-schardinger dextrin-doubly, adds beta-schardinger dextrin-weight 15-40 water doubly, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose;
The preferred technical scheme of described step (2) is:
Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 6-16 times of Cortex Cinnamomi weight, extraction time is 3-7 hour; The another device of aqueous solution after distillation is collected, and Cortex Cinnamomi medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 2 times of volumes, obtains volatile oil ethanol; Taking weight is the beta-schardinger dextrin-of 10 times of volatile oil volumes, adds the water of 25 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
4. according to the preparation method described in any one in claims 1 to 3, it is characterized in that, in described step (3), the concentration of volume percent of alcoholic solution I is 30%-80%, more preferably 70%;
Preferably, in described step (3), the volume of alcoholic solution I is the described Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae medical material gross weight 6-14 times; Preferred, the volume of alcoholic solution I is the described Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae medical material gross weight 10 times;
Preferably, in described step (3), extract 2-3 time each 0.5-2 hour; Preferred, extract each 1.5 hours 2 times.
5. according to the preparation method described in any one in claim 1 to 4, it is characterized in that, in described step (4), the weight of water is 6-16 times of medical material weight; Preferably, the weight of water is 8 times of medical material weight;
Preferably, in described step (4), water extraction 1-3 time, each 1-3 hour; Preferred, water extraction 2 times, each 2 hours.
6. according to the preparation method described in any one in claim 1 to 5, it is characterized in that, in described step (5), the concentration of volume percent of alcoholic solution II is 30%-80%; Preferred, the concentration of volume percent of alcoholic solution II is 60%;
Preferably, in described step (5), the volume of alcoholic solution II is 6-14 times of medical material weight; Preferred, the volume of alcoholic solution II is 10 times of medical material weight;
Preferably, in described step (5), extract 2-3 time each 0.5-2 hour; Preferred, extract each 1.5 hours 3 times.
7. preparation method according to claim 1, is characterized in that, the concrete operation step of described preparation method is as follows:
(1) according to described weight portion, prepare crude drug;
(2) Cortex Cinnamomi extraction by steam distillation volatile oil, the weight of water is 6-16 times of Cortex Cinnamomi weight, extraction time is 3-7 hour; The another device of aqueous solution after distillation is collected, and Cortex Cinnamomi medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 1-3 times of volume, obtains volatile oil ethanol; Taking weight is volatile oil volume 6-20 beta-schardinger dextrin-doubly, adds beta-schardinger dextrin-weight 15-40 water doubly, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose;
(3) the alcoholic solution I heating and refluxing extraction that the Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae are 30%-80% by the concentration expressed in percentage by volume that volume is medical material weight 6-14 times 2-3 time, each 0.5-2 hour, filter, merge ethanol extract each time, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1;
(4) the Cortex Cinnamomi medicinal residues that Fructus Mume and step (1) obtain, and step (2) Radix Astragali, Fructus Ligustri Lucidi and the Flos Buddlejae medicinal residues that obtain, with volume, be medical material weight 6-16 water heating and refluxing extraction doubly 1-3 time, each 1-3 hour, filters, merge filtrate each time, add the aqueous solution after the distillation that step (2) obtains, standing, filter, when filtrate is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2;
(5) Herba Leonuri, Rhizoma Coptidis are that the alcoholic solution II that medical material weight 6-14 concentration expressed in percentage by volume is doubly 30%-80% extracts 2-3 time with volume, each 0.5-2 hour, filter, merge ethanol extract each time, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 3;
(6) will extract extractum 1,2,3 and merge, spraying is dry, obtains dry extract, the described volatile oil clathrate compound that adds step (2) to obtain, and mix homogeneously, obtains;
The preferred concrete operation step of described preparation method is as follows:
(1) according to described weight portion, prepare crude drug;
(2) Cortex Cinnamomi extraction by steam distillation volatile oil, the another device of aqueous solution after distillation is collected, and Cortex Cinnamomi medicinal residues are standby; Volatile oil adds the anhydrous alcohol solution of 2 times of volumes, obtains volatile oil ethanol; Taking weight is the beta-schardinger dextrin-of 10 times of volatile oil volumes, adds the water of 25 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 1.5 hours, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose;
(3) the alcoholic solution I heating and refluxing extraction that the Radix Astragali, Fructus Ligustri Lucidi, Flos Buddlejae are 70% by the concentration expressed in percentage by volume that volume is 10 times of medical material weight 2 times, each 1.5 hours, filter, merge ethanol extract twice, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 1;
(4) the Cortex Cinnamomi medicinal residues that Fructus Mume and step (1) obtain, and step (2) Radix Astragali, Fructus Ligustri Lucidi and the Flos Buddlejae medicinal residues that obtain, with volume, be the water heating and refluxing extraction 2 times of 8 times of medical material weight, each 2 hours, filter, merge filtrate twice, add the aqueous solution after the distillation that step (2) obtains, standing, filter, when filtrate is concentrated into 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 2;
(5) the alcoholic solution II that Herba Leonuri, Rhizoma Coptidis are 60% by the concentration expressed in percentage by volume that volume is 10 times of medical material weight extracts 3 times, each 1.5 hours, filter, merge three times ethanol extract, reclaim ethanol, while being evaporated to 80 ℃, measure the extractum that relative density is 1.20-1.30, must extract extractum 3;
(6) will extract extractum 1,2,3 and merge, spraying is dry, obtains dry extract, the described volatile oil clathrate compound that adds step (2) to obtain, and mix homogeneously, obtains.
8. according to the preparation method described in any one in claim 1 to 7, it is characterized in that, described crude drug consists of:
Radix Astragali 30g, Fructus Ligustri Lucidi 15g, Herba Leonuri 15g, Fructus Mume 9g, Rhizoma Coptidis 6g, Cortex Cinnamomi 1g, Flos Buddlejae 6g.
9. the Chinese medicine extract that the preparation method described in claim 1 to 8 prepares.
10. the application in the medicine that Chinese medicine extract claimed in claim 9 becomes in preparation treatment of diabetic retinopathy; Preferably, acceptable adjuvant pharmaceutically described in described Chinese medicine extract adds or do not add, is prepared into acceptable preparation clinically.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105159074A (en) * | 2015-08-19 | 2015-12-16 | 四川九渊医药科技有限公司 | Optimization method for large-scale volatile oil extraction from medicinal materials |
| CN106214787A (en) * | 2016-09-20 | 2016-12-14 | 中国中医科学院西苑医院 | A kind of Chinese medicine composition treating diabetes and preparation method thereof and purposes |
| CN109925429A (en) * | 2019-04-16 | 2019-06-25 | 江西正邦动物保健品有限公司 | A kind of compound Chinese medicinal preparation and preparation method thereof improving sow reproductive performance |
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| CN1895399A (en) * | 2006-06-14 | 2007-01-17 | 高健生 | Chinese-medicinal preparation for treating early diabetic retinopathy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1895399A (en) * | 2006-06-14 | 2007-01-17 | 高健生 | Chinese-medicinal preparation for treating early diabetic retinopathy |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105159074A (en) * | 2015-08-19 | 2015-12-16 | 四川九渊医药科技有限公司 | Optimization method for large-scale volatile oil extraction from medicinal materials |
| CN105159074B (en) * | 2015-08-19 | 2017-08-29 | 四川九渊医药科技有限公司 | The optimization method of volatile oil in a kind of extensive extraction medicinal material |
| CN106214787A (en) * | 2016-09-20 | 2016-12-14 | 中国中医科学院西苑医院 | A kind of Chinese medicine composition treating diabetes and preparation method thereof and purposes |
| CN109925429A (en) * | 2019-04-16 | 2019-06-25 | 江西正邦动物保健品有限公司 | A kind of compound Chinese medicinal preparation and preparation method thereof improving sow reproductive performance |
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